US10759708B2 - High-light trasmittance zirconia sintered body, preparation method therefor and use thereof - Google Patents
High-light trasmittance zirconia sintered body, preparation method therefor and use thereof Download PDFInfo
- Publication number
- US10759708B2 US10759708B2 US16/289,369 US201916289369A US10759708B2 US 10759708 B2 US10759708 B2 US 10759708B2 US 201916289369 A US201916289369 A US 201916289369A US 10759708 B2 US10759708 B2 US 10759708B2
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- Prior art keywords
- zirconia
- powder
- sintered body
- aluminum oxide
- zirconia sintered
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 238000002360 preparation method Methods 0.000 title description 10
- 239000000843 powder Substances 0.000 claims abstract description 51
- 238000002834 transmittance Methods 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 20
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000002270 dispersing agent Substances 0.000 claims description 13
- 239000011230 binding agent Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 239000002002 slurry Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 150000003746 yttrium Chemical class 0.000 claims description 7
- 150000003754 zirconium Chemical class 0.000 claims description 7
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229920002635 polyurethane Polymers 0.000 claims description 5
- 239000004814 polyurethane Substances 0.000 claims description 5
- 229920000178 Acrylic resin Polymers 0.000 claims description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000004584 polyacrylic acid Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims 3
- 238000001035 drying Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 4
- 238000005245 sintering Methods 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 description 4
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000011351 dental ceramic Substances 0.000 description 1
- 239000005548 dental material Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 1
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 description 1
- 229920002523 polyethylene Glycol 1000 Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229910000347 yttrium sulfate Inorganic materials 0.000 description 1
- RTAYJOCWVUTQHB-UHFFFAOYSA-H yttrium(3+);trisulfate Chemical compound [Y+3].[Y+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RTAYJOCWVUTQHB-UHFFFAOYSA-H 0.000 description 1
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K6/00—Preparations for dentistry
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Definitions
- the present invention relates to the field of material engineering, specifically, to a high-light transmittance zirconia sintered body and preparation method therefor and use thereof.
- Zirconia ceramic is a new type of biomaterial with good biocompatibility and excellent mechanical properties, which has become the focus of dental ceramic development.
- CN104016677A discloses a light-transmissive zirconia sintered body and preparation method therefor.
- the zirconia for dental use prepared by the method has a relatively low transmittance, poor overall texture and jade-like appearance, is not aesthetically pleasing, and has certain limitations in application.
- ZL201010604330.3 discloses a dental high-transmittance zirconia material and preparation process thereof, which adopts a dry mixing process to prepare zirconia, prone to cause uneven distribution of strength and low strength of zirconia, and the ceramic sintered body is prone to cracking when applied.
- One purpose of the present invention is to provide a novel high-light transmittance zirconia sintered body and preparation method therefor.
- Another purpose of the present invention is to provide use of the high-light transmittance zirconia sintered body in the preparation of a fixed dental prosthesis.
- the present invention first provides a material for a high-light transmittance zirconia sintered body, and the material is prepared by the following method: adding an appropriate amount of water to zirconia powder and grinding, during which ⁇ -aluminum oxide powder is added, then spray granulating to obtain a powder material having an average particle diameter of 0.1 ⁇ m to 0.4 ⁇ m.
- the molar percentage of yttrium oxide in the zirconia powder is 4% to 6%.
- the ⁇ -aluminum oxide powder has a BET specific surface area of 5 to 16 m 2 /g.
- the zirconia powder has a BET specific surface area of 8 to 16 m 2 /g, and an average particle diameter of 0.1 to 0.4 ⁇ m.
- the preparation method of the zirconia powder is as follows:
- a soluble zirconium salt and a soluble yttrium salt are mixed at a ratio and dissolved in water, and ammonia water is slowly added under stirring to adjust the pH of the slurry to 8 to 10;
- the powder is subjected to heat treatment at 800 to 1200° C. for 2 to 5 h, and then grinding and dispersing;
- the dispersed particles are granulated to obtain a powder for a high-light transmittance zirconia sintered body
- the soluble zirconium salt includes zirconium oxychloride, zirconium nitrate, zirconium sulfate and the like; and the soluble yttrium salt includes yttrium chloride, yttrium nitrate, yttrium sulfate and the like.
- the molar ratio of the soluble zirconium salt to the yttrium salt is 94 to 96:4 to 6, preferably 95:5.
- a step of adding a dispersant and a binder to the mixture of the zirconia and the ⁇ -aluminum oxide is also included.
- the dispersant includes at least one selected from acrylic acid, polyacrylic acid, acrylamide, polyurethane and the like.
- the binder includes at least one selected from polyvinyl alcohol, polyethylene glycol, acrylic resin, carboxymethyl cellulose and the like.
- the weight parts of the feedstocks for preparing the material for the high-light transmittance zirconia sintered body of the present invention are as follows: 50 to 100 parts of zirconia powder, 0.01 to 0.1 parts of ⁇ -aluminum oxide powder, 0.1 to 0.5 parts of dispersant, 0.1 to 8.0 parts of binder, and 50 to 100 parts of water.
- the weight parts of the feedstocks are as follows: 100 parts of zirconia powder, 0.1 parts of ⁇ -aluminum oxide powder, 0.2 parts of dispersant, 5 parts of binder, and 100 parts of water.
- the material for the high-light transmittance zirconia sintered body of the present invention can be prepared by the following method: adding an appropriate amount of water to zirconia powder and grinding, during which ⁇ -aluminum oxide powder, water and alumina slurry are added and stirred for 5 to 30 minutes, then spray granulating to obtain a powder material having an average particle diameter of 0.1 ⁇ m to 0.4 ⁇ m for preparing a high-light transmittance zirconia sintered body.
- the present invention also provides a high-light transmittance zirconia sintered body prepared from the material.
- a ceramic with 1 mm thick of the sintered body has a linear transmittance of >47% and a three-point bending strength of >600 MPa.
- the obtained sintered body has a grain size of 0.1 to 0.7 ⁇ m, and a good toughness due to the dispersion and toughening by alumina. After the sintered body is aged at 140° C. for 20 h, the monoclinic phase of the aged sintered body is ⁇ 10%, and the anti-aging property is excellent.
- the high-light transmittance zirconia sintered body of the present invention can be prepared by the following method: the material for a high-light transmittance zirconia sintered body is processed and molded, and then subjected to high-temperature sintering in the atmosphere under normal pressure. For example, the temperature for high-temperature sintering is maintained at 1400 to 1550° C. for 1 to 4 h.
- the present invention also provides the use of the high-light transmittance zirconia sintered body in the preparation of a fixed dental prosthesis (including a denture).
- the present invention further provides a fixed dental prosthesis, such as zirconia denture, prepared from the high-light transmittance zirconia sintered body.
- a fixed dental prosthesis such as zirconia denture
- the zirconia sintered body provided by the present invention has a grain size of 0.1 to 0.7 ⁇ m, and the zirconia sintered body has a higher strength and toughness due to the dispersion and toughening by aluminum oxide. Pores in the zirconia powder can be eliminated by adding aluminum oxide.
- the zirconia sintered body has a higher light transmittance, and the prepared dentures have good texture, good jade-like appearance, and are closer to the human teeth.
- the percent sign “%” involved in the present invention means a percentage by mass unless otherwise specified. However, the percentage of a solution, unless otherwise specified, means the number of grams of the solute contained in 100 mL solution.
- the ⁇ -aluminum oxide powder used in the following Examples has a BET specific surface area of 5 to 16 m 2 /g.
- Examples 1 to 5 Material for a High-Light Transmittance Zirconia Sintered Body
- the material for the high-light transmittance zirconia sintered body of the present invention can be prepared by the following method: adding an appropriate amount of water to zirconia powder and grinding, during which ⁇ -aluminum oxide powder is added, and then the powder material having an average particle diameter of 0.1 to 0.4 ⁇ m for preparing the high-light transmittance zirconia sintered body was obtained by spray granulation. (Table 1)
- Example 1 Example 2
- Example 3 Example 4
- Example 5 Molar percentage of 4.5 5.3 6 5 5 yttrium oxide in zirconia powder
- BET specific surface area 10-16 10-16 10-16 10-16 10-16 of zirconia powder, m 2 /g Average particle diameter 0.1-0.4 0.1-0.4 0.1-0.4 0.1-0.4 of zirconia powder, ⁇ m Dispersant Acrylic acid Polyacrylic Polyacrylic Acrylamide Polyurethane acid acid Binder PEG 1000 PVA124 PVA205 PEG400 PVA105 Weight ratio of zirconia 100:0.1:0.4:2:80 50:0.05:0.1:0.5:100 100:0.1:0.2:5:100 100:0.1:0.3:8:80 100:0:0.5:3:50 powder, ⁇ -aluminium oxide powder, dispersant, binder and water Average particle diameter 0.210 0.198 0.202 0.321 0.189 of the material for the high-light transmittance zirconia sintered body,
- the preparation method of the zirconia powder was as follows:
- the slurry was transferred to a reaction kettle, and subjected to hydrothermal synthesis at 140 to 200° C. for 10 to 72 h;
- the powder was subjected to heat treatment at 800 to 1200° C. for 2 to 5 h, and then grinding and dispersing;
- the dispersed particles were granulated to obtain a powder for a high-light transmittance zirconia sintered body.
- the powder prepared in Examples 1 to 5 was subjected to dry-pressing molding (molding pressure: 150 to 250 MPa), and then sintering at 1400 to 1550° C. in the atmosphere under normal pressure for 1 to 4 h to obtain the high-light transmittance zirconia sintered body.
- the various indexes of the obtained sintered body products were shown in Table 2.
- Example 6 Example 7
- Example 8 Example 9
- the high-light transmittance zirconia sintered body provided in the present invention can be used as dental materials such as fixed dental prostheses, for example, dentures.
- the zirconia sintered body provided in the present invention has a grain size of 0.1 to 0.7 ⁇ m, and due to the dispersion and toughening by aluminum oxide, the zirconia sintered body has a higher strength and toughness. Pores in the zirconia powder can be eliminated by adding aluminum oxide.
- the zirconia sintered body has a higher light transmittance, and the prepared dentures have good texture, good jade-like appearance, and are closer to the human teeth.
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Abstract
Description
TABLE 1 |
Powder for the high-light transmittance zirconia sintered body |
Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | ||
Molar percentage of | 4.5 | 5.3 | 6 | 5 | 5 |
yttrium oxide in zirconia | |||||
powder | |||||
BET specific surface area | 10-16 | 10-16 | 10-16 | 10-16 | 10-16 |
of zirconia powder, m2/g | |||||
Average particle diameter | 0.1-0.4 | 0.1-0.4 | 0.1-0.4 | 0.1-0.4 | 0.1-0.4 |
of zirconia powder, μm | |||||
Dispersant | Acrylic acid | Polyacrylic | Polyacrylic | Acrylamide | Polyurethane |
acid | acid | ||||
Binder | PEG 1000 | PVA124 | PVA205 | PEG400 | PVA105 |
Weight ratio of zirconia | 100:0.1:0.4:2:80 | 50:0.05:0.1:0.5:100 | 100:0.1:0.2:5:100 | 100:0.1:0.3:8:80 | 100:0:0.5:3:50 |
powder, α-aluminium | |||||
oxide powder, dispersant, | |||||
binder and water | |||||
Average particle diameter | 0.210 | 0.198 | 0.202 | 0.321 | 0.189 |
of the material for the | |||||
high-light transmittance | |||||
zirconia sintered body, μm | |||||
TABLE 2 |
Indexes of high-light transmittance zirconia sintered body products |
Example 6 | Example 7 | Example 8 | Example 9 | Example 10 | ||
Linear transmittance of 1 mm thick | 47 | 50 | 48 | 47 | 49 |
ceramic, % | |||||
Three-point bending strength, MPa | 750 | 820 | 648 | 800 | 748 |
Monoclinic phase of the aged | 7.6 | 5.3 | 1.2 | 2.5 | 2.8 |
sintered body, % | |||||
Fracture toughness, MPa · m1/2 | 7 | 9 | 8 | 6 | 6 |
Claims (10)
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CN201610793366.8A CN106431395A (en) | 2016-08-31 | 2016-08-31 | High-light transmittance zirconia sintered body, and preparation method and application thereof |
CN201610793366.8 | 2016-08-31 | ||
CN201610793366 | 2016-08-31 | ||
PCT/CN2017/095747 WO2018040835A1 (en) | 2016-08-31 | 2017-08-03 | High-light transmittance zirconia sintered body, preparation method therefor and use thereof |
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CN106396676A (en) * | 2016-08-31 | 2017-02-15 | 山东国瓷功能材料股份有限公司 | Light transmittance zirconium oxide sintered body, preparation method and application thereof |
CN106431395A (en) * | 2016-08-31 | 2017-02-22 | 山东国瓷功能材料股份有限公司 | High-light transmittance zirconia sintered body, and preparation method and application thereof |
CN110891920A (en) * | 2017-07-31 | 2020-03-17 | 可乐丽则武齿科株式会社 | Method for manufacturing powder comprising zirconium oxide particles and fluorescent agent |
CN110891921A (en) * | 2017-07-31 | 2020-03-17 | 可乐丽则武齿科株式会社 | Zirconia sintered body containing fluorescent agent |
CN110891903A (en) * | 2017-07-31 | 2020-03-17 | 可乐丽则武齿科株式会社 | Method for producing powder containing zirconia particles |
CN107759218B (en) * | 2017-12-11 | 2020-06-16 | 内蒙古科技大学 | Yttria-stabilized zirconia ceramic and preparation method thereof |
KR102692692B1 (en) * | 2019-03-06 | 2024-08-06 | 쿠라레 노리타케 덴탈 가부시키가이샤 | Zirconia sintered body with high straight light transmittance |
WO2020218541A1 (en) * | 2019-04-25 | 2020-10-29 | クラレノリタケデンタル株式会社 | Zirconia calcined body suitable for dental use and method for manufacturing same |
US11661650B2 (en) * | 2020-04-10 | 2023-05-30 | Applied Materials, Inc. | Yttrium oxide based coating composition |
CN114014652A (en) * | 2021-11-08 | 2022-02-08 | 长裕控股集团有限公司 | Low-temperature sintered zirconia ceramic and preparation process thereof |
CN116409990A (en) * | 2021-12-31 | 2023-07-11 | 万华化学集团股份有限公司 | Zirconia ceramic and preparation method thereof |
CN116023164B (en) * | 2023-03-29 | 2023-06-06 | 湖南康纳新材料有限公司 | Porous zirconia ceramic block for dental restoration and preparation method and application thereof |
CN118545995B (en) * | 2024-07-29 | 2024-10-11 | 湖南泽尔顿新材料有限公司 | Preparation method of ultra-high permeability zirconia powder |
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US20190210927A1 (en) | 2019-07-11 |
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